• Title/Summary/Keyword: trace impurity

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Reuse of Eluent by Controlling its Specific Gravity during the Chromatographic Purification of Paclitaxel (크로마토그래피를 이용한 Paclitaxel 정제에서 비중 조절에 의한 Eluent 재사용)

  • Kim, Jin-Hyun
    • KSBB Journal
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    • v.22 no.5
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    • pp.366-369
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    • 2007
  • In this study, the feasibility of reusing the eluent was confirmed by monitoring its specific gravity during the chromatographic purification of paclitaxel from plant cell cultures. The specific gravity of the eluent (methanol/water = 70/30, v/v) was measured prior to its elution through the hydrophobic resin column. The measurement showed a specific gravity of 0.853. The discharged eluent from the column outlet was first evaporated under vacuum pressure. The evaporated eluent was collected and condensed into a liquid eluent again, followed by the HPLC analysis in order to check the presence of any trace of impurity. Even if the specific gravity of the liquid eluent is varied from 0.853 as a result of the evaporation and condensation, the eluent can still be reused after it specific gravity is adjusted by the addition of methanol or water. The reuse of the eluent resulted in the paclitaxel yield of 86% with a purity of 95% which were closely similar to those of before the eluent reuse. These results indicate that the strategy of reusing the eluent on the basis of the specific gravity analysis was successfully implemented in this study.

Recovery of Metallic Lithium by Room-Temperature Electrolysis: I. Effect of Electrode Materials (상온(常溫) 전해법(電解法)에 의한 리튬 금속(金屬)의 회수(回收): I. 전극물질(電極物質)의 영향(影響))

  • Lee, Jae-O;Park, Jesik;Lee, Churl Kyoung
    • Resources Recycling
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    • v.21 no.6
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    • pp.45-50
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    • 2012
  • The room-temperature electrodeposition of metallic lithium was investigated from ionic liquid, 1-methyl-1-propylpiperidinium bis(trifluoromethanesulfonyl)imide (PP13TFSI) with lithium bis (trifluoromethanesulfonyl)imide (LiTFSI) as a lithium source. Cyclic voltammograms on gold working electrode showed the possibility of the electrodeposition of metallic lithium, and the reduction current on a gold electrode was higher than the value on platinum and copper. The metallic lithium could be electrodeposited on the gold electrode under potentiostatic condition at -2.4 V (vs. Pt-QRE) and was confirmed by analytical techniques including XRD and SEM-EDS. The dendrite-typed electrodeposits were composed of a metallic lithium and a alloy with gold substrate. And any impurity could be detected except for trace oxygen introduced during handling for the analyses.

Recovery of Silicon from Silicon Sludge by Electrolysis (실리콘 슬러지로부터 실리콘의 전해회수(電解回收))

  • Park, Jesik;Jang, Hee Dong;Lee, Churl Kyoung
    • Resources Recycling
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    • v.21 no.5
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    • pp.31-37
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    • 2012
  • As a recovery of elemental silicon from the sludge of Si wafer process, a process of mechanical separation-chlorine roasting-electrolysis has been suggested. The silicon sludge consisted of Si, SiC, machine oil, and metallic impurities. The oil and metal impurities was removed by mechanical separation. The Si-SiC mixture was converted to silicon chloride by chlorine roasting at $1000^{\circ}C$ for 1 hr and the silicon chloride was dissolved into an ionic liquid of $[Bmpy]Tf_2N$ as an electrolyte. Cyclic voltammetry results showed an wide voltage window of pure $[Bmpy]Tf_2N$ and a reduction peak of elemental Si from $[Bmpy]Tf_2N$ dissolved $SiCl_4$ on Au electrode, respectively. The silicon deposits could be prepared on the Au electrode by the potentiostatic electrolysis of -1.9 V vs. Pt-QRE. The elemental silicon uniformly electrodeposited was confirmed by various analytical techniques including XRD, FE-SEM with EDS, and XPS. Any impurity was not detected except trace oxygen contaminated during handling for analysis.

Background effect on the measurement of trace amount of uranium by thermal ionization mass spectrometry (열이온화 질량분석에 의한 극미량 우라늄 정량에 미치는 바탕값 영향)

  • Jeon, Young-Shin;Park, Yong-Joon;Joe, Kih-Soo;Han, Sun-Ho;Song, Kyu-Seok
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.487-494
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    • 2008
  • An experiment was performed for zone refined Re-filament and normal (nonzone refined) Re-filament to reduce the background effect on the measurement of low level uranium samples. From both filaments, the signals which seemed to come from a cluster of light alkali elements, $(^{39}K_6)^+$, $(^{39}K_5+^{41}K)^+$ and $PbO_2$ were identified as the isobaric effect of the uranium isotopes. The isobaric effect signal was completely disappeared by heating the filament about $2000^{\circ}C$ at < $10^{-7}$ torr of vacuum for more than 1.5 hour in zone refined Refilaments, while that from the normal Re-filaments was not disappeared completely and was still remained as 3 pg. of uranium as the impurities after the degassing treatment was performed for more than 5 hours at the same condition of zone refined filaments. A threshold condition eliminating impurities were proved to be at 5 A and 30 minutes of degassing time. The uranium content as an impurity in rhenium filament was checked with a filament degassing treatment using the U-233 spike by isotope dilution mass spectrometry. A 0.31 ng of U was detected in rhenium filament without degassing, while only 3 pg of U was detected with baking treatment at a current of 5.5 A for 1 hr. Using normal Re-filaments for the ultra trace of uranium sample analysis had something problem because uranium remains to be 3 pg on the filament even though degassed for long hours. If the 1 ng uranium were measured, 0.3% error occurred basically. It was also conformed that ionization filament current was recommended not to be increased over 5.5 A to reduce the background. Finally, the contents of uranium isotopes in uranium standard materials (KRISS standard material and NIST standard materials, U-005 and U-030) were measured and compared with certified values. The differences between them showed 0.04% for U-235, 2% for U-234 and 2% for U-236, respectively.

Analysis of Heavy Metals in $[^{201}Tl]$TICI Injection Using Polarography (폴라로그래피를 이용한 $[^{201}Tl]$염화탈륨 주사액의 중금속 분석)

  • Chun, Kwon-Soo;Suh, Yong-Sup;Yang, Seung-Dae;Ahn, Soon-Hyuk;Kim, Sang-Wook;Choi, Kang-Hyuk;Lee, Dong-Hoon;Lim, Sang-Moo;Yu, Kook-Hyun
    • The Korean Journal of Nuclear Medicine
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    • v.34 no.4
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    • pp.336-343
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    • 2000
  • Purpose: Thallous-201 chloride produced at Korea Cancer Center Hospital(KCCH) is used in detecting cardiovascular disease and cancer. Thallium impurity can cause emesis, catharsis and nausea, so the presence of thallium and other metal impurities should be determined. According to USP and KP, their amounts must be less than 2 ppm in thallium and 5 ppm in total. In this study, the detection method of trace amounts of metal impurities in $[^{201}Tl]$TICI injection with polarography was optimized without environmental contamination. Materials and Methods: For the detection of metal impurities, Osteryoung Square Wave Stripping Voltammetry method was used in Bio-Analytical System (BAS) 50W polarograph. The voltammetry was composed of Dropping Mercury Electrode (DME) as a working electrode, Ag/AgCl as a reference electrode and Pt wire as a counter electrode. Square wave stripping method, which makes use of formation and deformation of amalgam, was adopted to determine the metal impurities, and pH 7 phosphate buffer was used as supporting electrolyte. Results: Tl, Cu and Pb in thallous-201 chloride solution were detected by scanning from 300 mV to -800 mV Calibration curves were made by using $TINO_3,\;CuSO_4\;and\;Pb(NO_3){_2}$ as standard solutions. Tl was confirmed at -450 mV peak potential and Cu at -50 mV Less than 2 ppm of Tl and Cu was detected and Pb was not detected in KCCH-produced thallous-201 chloride injection. Conclusion: Detection limit of thallium and copper is approximately 50 ppb with this method. As a result of this experiment, thallium and other metal impurities in thallous-201 chloride injection, produced at Korea Cancer Center Hospital, are in the regulation of USP and KP Polarograph could be applied for the determination of metal impurities in the quality control of radiopharmaceuticals conveniently without environmental contamination.

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